Synthesis of Chloral Hydrate

by Smoothe

Please note that Chloral Hydrate is a schedule IV controlled substance in the US and following the below synth without the proper knowledge and permits
would thus constitue a criminal act.

This a very easy synth with all chemicals needed being very easily obtainable from your local grocery store (Sani-flush, bleach), liquor store (grain
alcohol "gem clear") and hardware store (Sulfuric acid drain cleaner). As far as the calcium oxide used in the last steps I'm not sure this is really a
necessary step other than producing a more pure product. I think that if someone were to stop at step 18 the Chloral Hydrate would have a high enough
purity for consumption.

If you have any comments or suggestions for this synth please post them to Smoothe@hotmail.com

Visitors have pointed out that this procedure results in extremely poisonous chlorine gas with possible unknown contaminants from the use of over the counter commercial products that might change formulation over time. Inhalation of chlorine gas is potentially lethal and at sub fatal levels can scar and damage the eyes, throat, and lungs. In laboratory settings, chlorine gas would not be synthesized without complex gas containment equipment. This technique should be considered fundamentally unsafe as a home method. (Erowid March 29, 2014)

Procedure

Put 350ml of anhydrous alcohol (Dry or distill pure grain alcohol.) into a 600ml flask and put a 2-hole stopper into the top.

Put 2" of bleach and 1 tsp. 'Sani-flush' into a clean 500ml flask and put a 2-hole stopper into the top.

Attach a fish tank aerator to the flask in step 2 by a lenght of plastic tubing and inserting this tubing into the top of the stopper.

Connect the remaining opening of the flask in step 2 to one of the openings on the flask in step 1 using another piece of plastic tubing.

Place a piece of glass tubing long enough to reach the bottom of the flask in step 1 and insert it into the tubing in step 4 so that it reaches into
the bottom of the alcohol flask. (This should start the bubbling of chlorine gas through the alcohol.)

Place another piece of plastic tubing into the remaining opening of the alcohol flask and put the open end into the bottom of a 500ml flask.

Place the 500ml flask in step 6 in a cold water bath.

Continue to bubble the chlorine gas through the alcohol until it will absorb no more gas.

Gently heat the alcohol flask using a water bath until the alcohol begins to boil. (Some of the alcohol will distill off into the flask in step 6,
several times during the chlorinating process pour the alcohol that distills back into the alcohol flask into the alcohol flask.)

When the flask is totally chlorinated it is poured into a pyrex dish and allowed to cool. (If the above steps were done properly you should have a
large mass of crystals upon cooling.)

Pour concentrated sulfuric acid equal to 3 times the volume of the impure Chloral Hydrate (the crystal mass) into the dish.

Heat this dish on a water bath until the Chloral Hydrate crystals are melted, this soultion should then be stirred for approx. 3 min.

Pour the solution from step 12 back into a clean dry 1000ml flask and heat (Do not heat above 200F.)

As the solution in step 13 heats up the still impure Chloral Hydrate will begin to float to the surface, when it stops rising use a basting syringe
(Or whatever you prefer.) to draw off the floating layer of Chloral and place this into a clean, dry beaker.

Repeat step 14 until no more Chloral rises to the surface.

Heat the beaker in the above step 14 to around 190F for 20 min. to get rid of any alcohol or acid remaining in this solution.

Pour the solution from step 16 back into the flask in step 13 (1000ml flask) and add an equal amount (by volume) of sulfuric acid to this flask and
stir for approx. 5 min.

Distill off the Chloral Hydrate (which distills at 210F) into a clean dry beaker that is placed in an ice bath. (This should not be hard as the
sulfuric acid distills at 722F.)

Place the distilled Chloral from the above step back into a cleaned, dry 500ml flask and add an equal amount (by volume) of calcium oxide to this flask.

Once again distill off the Chloral until the surface of the calcium oxide is dry.

To use the Chloral Hydrate you have just made add one part water to two parts (by volume) of finished product. The dose range is 250mg-1000mg. Add the
desired amount of Chloral solution to a drink of your choice and drink up. Choose a drink to add this to that will mask the taste of the Chloral as it has
a bitter taste. Onset is in about 15 min-30 min. (And you or whoever has taken this will be out for the night.)